Abstract: | The local structures of pure NiAl and Ti‐, Co‐doped NiAl compounds have been obtained utilizing extended X‐ray absorption fine‐structure (EXAFS) spectroscopy. The results provide experimental evidence that Ni antisite defects exist in the Ni‐rich NiAl compounds. The site preference of Ti and Co has been confirmed. Ti occupies the Al sublattice, while Co occupies the Ni sublattice. The structure parameters obtained by EXAFS were consistent with the X‐ray diffraction results. Owing to the precipitation of α‐Cr, the local structure of NiAl‐Cr has not been obtained, making the site preference of Cr unclear. |